TY - CONF A1 - Matschat, Ralf T1 - CCQM-K42 and P34.1: Constituents of an Al alloy T2 - CCQM Inorganic Analysis Working Group, CENAM (Centro Nacional de Metrología) CY - Querétaro, Mexico DA - 2004-10-27 PY - 2004 AN - OPUS4-4407 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - High Purity Metals used as Primary Pure Calibration Materials: State of Development and Multielement Trace Determination in Zinc and Gold by HR ICP-MS T2 - 11th International Conference on Ultra-High Purity Base Metals, NIST (National Institute of Standards and Technology) CY - Gaithersburg, MD, USA DA - 2004-12-06 PY - 2004 AN - OPUS4-4630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - CCQM-P62: Purity analysis of nickel T2 - CCQM Inorganic Analysis Working Group, CENAM (Centro Nacional de Metrología) CY - Querétaro, Mexico DA - 2004-10-27 PY - 2004 AN - OPUS4-5969 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Czerwensky, Michael A1 - Matschat, Ralf T1 - ICP-MS analysis of high purity molybdenum used as SI-traceable standard of high metrological quality N2 - The need, concept and technical approach for the certification of SI-traceable standards of high metrological quality for chemical analysis of the elements is briefly explained. As an example of problems occurring in the certification of these standards, special technical aspects related to the analysis of high purity Mo by ICP-MS, namely blank reduction for Na, Li and Ni by protective coating of the cones with silicon, as well as dealing with the interferences from the Mo matrix, are discussed. PY - 2005 UR - http://cat.inist.fr/?aModele=afficheN&cpsidt=16469686 SN - 0267-9477 SN - 1364-5544 VL - 20 IS - 1 SP - 28 EP - 34 PB - Royal Society of Chemistry CY - London AN - OPUS4-5483 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - Multielement-Spurenbestimmung mit magnetisch stabilisierter Bogenanregung und optischer Emissionsspektrometrie T2 - Anwenderseminar direkte Feststoff-OES CY - Kempten, Germany DA - 2004-05-24 PY - 2004 AN - OPUS4-5496 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matschat, Ralf A1 - Kipphardt, Heinrich T1 - Das Primäre Kalibriersystem der BAM für die Elementanalytik PY - 2003 SN - 0044-2658 IS - 4 SP - 179 EP - 189 PB - Gesellschaft Deutscher Metallhütten- und Bergleute CY - Clausthal-Zellerfeld AN - OPUS4-6187 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emons, H. A1 - Marriott, J. A1 - Matschat, Ralf T1 - ERM - A new landmark for reference materials KW - Europäische Referenzmaterialien KW - Europäische Zusammenarbeit PY - 2005 DO - https://doi.org/10.1007/s00216-004-2844-2 SN - 1618-2642 SN - 1618-2650 VL - 381 IS - 1 SP - 28 EP - 29 PB - Springer CY - Berlin AN - OPUS4-7300 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - EUROMET Project 724: Sulfur in fuel - Improvement of existing IDMS procedures T2 - EUROMET-METCHEM Meeting CY - Sofia, Bulgaria DA - 2004-02-10 PY - 2004 AN - OPUS4-7703 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matschat, Ralf A1 - Heinrich, Hans-Joachim A1 - Czerwensky, Michael A1 - Kuxenko, Sandra A1 - Kipphardt, Heinrich T1 - Multielement trace determination in high purity advanced ceramics and high purity metals T2 - International Symposium on Ultrapure Materials (ISUPM) CY - Hyderabad, India DA - 2004-11-22 KW - Advanced ceramics KW - Pure metals KW - SS ET AAS KW - HR ICP-MS PY - 2005 SN - 0250-4707 SN - 0973-7669 VL - 28 IS - 4 SP - 361 EP - 366 PB - Indian Academy of Sciences CY - Bangalore AN - OPUS4-10889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Schiel, D. A1 - Rienitz, O. T1 - Primäre Kalibriermaterialien für die Elementanalytik PY - 2003 DO - https://doi.org/10.1002/nadc.20030510714 SN - 1439-9598 SN - 1521-3854 VL - 51 IS - 7/8 SP - 827 EP - 829 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-2582 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - BAM System of Primary Pure Elements - Aim and Current State T2 - Annual Meeting of Inorganic Working Group of CCQM CY - Ottawa, Canada DA - 2002-10-09 PY - 2002 AN - OPUS4-3713 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - Current State-Progress Report of the CCQM Pilot Study P34 "Aluminium Alloy" T2 - Annual Meeting of Inorganic Working Group of CCQM CY - Ottawa, Canada DA - 2002-10-09 PY - 2002 AN - OPUS4-3714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - Metrologische Aktivitäten der Fachgruppe I.1 der BAM T2 - Expertentreffen BAM-PTB CY - Braunschweig, Germany DA - 2002-11-04 PY - 2002 AN - OPUS4-3715 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - Activities of Division "Inorganic Chemical Analysis; Reference Materials" of BAM in the field Analysis of Materials T2 - The International Symposium on the Progress in Metal Science CY - Tokyo, Japan DA - 2002-10-17 PY - 2002 AN - OPUS4-2938 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - Multielement trace determination in high purity advanced ceramics and in high purity metals (invited talk) N2 - Multielement trace determination in high purity advanced ceramics and in high purity metals Ralf Matschat, Hans-Joachim Heinrich, Michael Czerwensky, Sandra Kuxenko and Heinrich Kipphardt Federal Institute for Materials Research and Testing (BAM), Richard-Willstaetter-Strasse 11, D-12489 Berlin, Germany Certified reference materials (CRMs) are of high importance to check the trueness of results in chemical analysis. In the field of advanced ceramics two CRMs were developed in the last years by the Federal Institute for Materials Research and Testing - (BAM), one for silicon nitride and one for silicon carbide. The certification of these materials is briefly discussed in this contribution. Both CRMs are not of extremely high purity in the classical sense, but besides their application by industry they are appropriate to be used for the validation of special methods used for trace determination in accordant high purity materials. This is demonstrated for the example of ultrapure silicon carbide which was analyzed by solid sampling electrothermal atomic absorption spectrometry (SS ET AAS). Wet chemical dissolution of this pure material typically introduces blanks which are too high for ultratrace analysis. Therefore SS ET AAS as a direct method was applied which does not need any wet chemical sample preparation. This method can be applied very effectively concerning sample throughput. But, as for all direct solid sampling methods, the calibration is a problem difficult to solve. By using the accordant CRM it could be demonstrated, that the calibration with liquid sample aliquots can be performed without affecting the trueness of the results. The analytical parameters and the performance of the method are discussed. Besides the so-called matrix CRMs, as reported for silicon nitride and silicon carbide, BAM is also certifying primary pure reference materials used as the National Standards for inorganic analysis in Germany. This work is performed in the frame of an extensive project in co?operation with the sister institute of BAM, the Physikalisch Technische Bundesanstalt (PTB). The crucial point of this project is the certification of the purity of high purity materials, each representing one element of the periodic table. Up to now more than ten primary CRMs are certified or not far from being certified. A variety of different analytical methods was necessary to determine the trace contents of metallic and non-metallic impurities from almost the whole periodic table in the high purity materials. Using high purity copper as an example the application and the results of the different methods applied are demonstrated. Another example presented is high purity iron. In this context the very good comparability of the results from two different methods, used for the determination of metallic traces is demonstrated. One of these methods was the "working horse" - the sector field high resolution ICP mass spectrometry (HR ICP-MS) mainly used in low resolution mode to exploit the good detection power and the other one was the electrothermal atomic absorption spectrometry (ET AAS), which was used to confirm the results of the HR ICP-MS. The analysis of pure molybdenum is presented as a third example. The problems of spectral matrix interference are discussed and different ways of their handling are pointed out. By this example it can also be demonstrated, how the coating of the inlet cones of the ICP mass spectrometer by matrix elements of solutions - which normally is an adverse effect - can be advantageously used to decrease the measured blank values of some analyte elements drastically. T2 - International Symposium on "Ultrapure Materials: Processing, Characterization and Applications" CY - Hyderabad, India DA - 2004-11-22 PY - 2004 AN - OPUS4-4055 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dette, Angelika A1 - Guadagnino, E. A1 - Matschat, Ralf A1 - Sundberg, P. T1 - Certification of the mass fractions of total and hexavalent chromium in glass: a joint collaborative work in co-operation with BAM and ICG KW - Glasreferenzmaterial KW - Hexavalentes Chrom KW - Verpackungsverordnung PY - 2004 SN - 0391-4259 IS - 1 SP - 5 EP - 14 PB - Aurora Pubbl. CY - Venezia AN - OPUS4-11868 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rienitz, O. A1 - Jährling, R. A1 - Schiel, D. A1 - Matschat, Ralf A1 - Kipphardt, Heinrich A1 - Gernand, W. A1 - Oeter, D. T1 - Rückführung in der Elementanalytik PY - 2005 SN - 0030-834X VL - 115 IS - 4 SP - 295 EP - 299 PB - Wirtschaftsverl. NW CY - Bremerhaven AN - OPUS4-12056 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Rienitz, O. A1 - Schiel, D. A1 - Gernand, W. A1 - Oeter, D. T1 - Traceability system for elemental analysis N2 - A complete metrological traceability system for measurement results of chemical analysis was set up. Core components are pure substances (national standards) characterised at the highest metrological level, primary solutions prepared from these pure substances and secondary solutions deduced from the primary solutions and intended for sale. The relative uncertainty of the element mass fraction of the primary substances and solutions is < 0.01 and < 0.05%, respectively. For the certification of transfer solutions and for stability testing, a precision measurement method for element contents has been developed by means of optical emission spectrometry (ICP OES) by which uncertainties between 0.1 and 0.05% can be achieved. The dissemination to field laboratories is effected with the aid of a calibration laboratory of the German Calibration Service (DKD) which certifies the element content of the secondary solutions with an uncertainty <= 0.3%. Calibration with these solutions enables the user to establish traceability of his measurement results to the International System of Units (SI). Currently, the system comprises Cu, Fe, Bi, Ga, Si, Na, K, Sn, W, and Pb. KW - Elemental analysis KW - Traceability KW - Elemental calibration solutions KW - Pure substances KW - Precision measurement of elements PY - 2006 DO - https://doi.org/10.1007/s00769-005-0084-6 SN - 0949-1775 SN - 1432-0517 VL - 10 IS - 11 SP - 633 EP - 639 PB - Springer CY - Berlin AN - OPUS4-12199 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - Netzwerk "Metrologie in der Chemie" für zuverlässige Messergebnisse in der chemischen Analytik T2 - Analytica Conference CY - Munich, Germany DA - 2006-04-25 PY - 2006 AN - OPUS4-12146 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hioki, A. A1 - Kurahashi, M. A1 - Turk, G. A1 - Matschat, Ralf A1 - Recknagel, Sebastian T1 - CCQM-K33 Final Report - Determination of minor elements in steel N2 - The key comparison CCQM-K33 was organized by the Inorganic Analysis Working Group of the CCQM to test the abilities of the national metrology institutes to measure the mass fractions of minor elements in steel. Elements to be analysed were Cr, Mn, Ni and Mo in low alloy steel. The National Metrology Institute of Japan (NMIJ), the National Institute of Standards and Technology (NIST) and the Federal Institute for Materials Research and Testing (BAM) acted as the coordinating laboratories. The participants used various measurement methods, though many of them used ICP-AES. Generally speaking, the agreement of the results was very good for each measurand. PY - 2006 DO - https://doi.org/10.1088/0026-1394/43/1A/08007 SN - 0026-1394 SN - 1681-7575 VL - 43 IS - Technical Supplement 1A 08007 SP - 1 EP - 15 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-12349 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matschat, Ralf A1 - Hinrichs, J. A1 - Kipphardt, Heinrich T1 - Application of glow discharge mass spectrometry to multielement ultra-trace determination in ultrahigh-purity copper and iron: a calibration approach achieving quantification and traceability N2 - A new approach was developed for quantitative calibration in GD-MS which can afford reliable and metrologically traceable results for many trace elements and was exemplified for pure copper and pure iron. It can be assumed that the technique can be further improved and applied to the analysis of other pure metals. Pressed copper and iron powder samples were used to calibrate the glow discharge mass spectrometry applied to the analysis of pure copper and iron. The new type of glow discharge mass spectrometer—the Element GD (Thermo Electron Corporation)—was used with a Grimm-type discharge cell for flat samples. Two series of powder samples were prepared for each of the copper and iron matrixes. The powders were quantitatively doped with solutions of graduated and defined concentrations of 40 or 20 analytes, respectively. The mass fractions of the analytes in the dried and homogenized metal powder samples ranged from µg/kg levels up to 10 mg/kg levels. A special technique was developed to press the samples and to form mechanically stable pellets with low risk of contamination. Ion beam ratios of analyte ions to matrix ions were used as measurands. The calibration curves were determined and the linear correlation coefficients were calculated for different intervals of the curves. The linear correlation coefficients are very satisfactory for most of the calibration curves, which include the higher segments of mass fractions; however, they are less satisfactory for the lower segments of the calibration curves. Nevertheless, in many cases rather acceptable and rather promising values were achieved even for these lower segments, representing mass fractions of analytes at ultra-trace level. The comparison of the certified values of different reference materials with the measured values based on calibrations with the pressed powder samples led to deviations less than 30% for most of the considered examples. KW - Glow discharge mass spectrometry (GD-MS) KW - High-purity copper KW - High-purity iron KW - Doped and pressed metal powder samples KW - Grimm-type cell KW - Metrological traceability PY - 2006 DO - https://doi.org/10.1007/s00216-006-0645-5 SN - 1618-2642 SN - 1618-2650 VL - 386 IS - 1 SP - 125 EP - 141 PB - Springer CY - Berlin AN - OPUS4-12649 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - Application of Glow Discharge Mass Spectrometry to the Multielement Ultra-Trace Determination in Ultrahigh Purity Copper and Iron - a Way of Calibration to Achieve Qualification and Traceability T2 - International Conference on Ultrahigh Purity Base Metals, UHPM 2005 CY - Nagasaki, Japan DA - 2005-11-07 PY - 2005 AN - OPUS4-10953 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guadagnino, E. A1 - Matschat, Ralf A1 - Dette, Angelika A1 - Sundberg, P. T1 - Certification of the mass fractions of trace elements in glass to be used for multi-element determination by XRF: a joint collaborative work in cooperation between BAM and ICG KW - Glasreferenzmaterial KW - Röntgenfluoreszenzanalyse KW - Multielementspurenbestimmung PY - 2005 SN - 0391-4259 IS - 4 SP - 5 EP - 16 PB - Aurora Pubbl. CY - Venezia AN - OPUS4-11665 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - The importance of well characterized high-purity metals in the field of analytical chemistry - first attempt of international harmonization at highest metrological level T2 - 13th International Conference on ultra high-purity base metals, BAM CY - Berlin, Germany DA - 2006-09-11 PY - 2006 AN - OPUS4-13486 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Hans-Joachim A1 - Pattberg, S. A1 - Barrault, Eric A1 - Matschat, Ralf ED - Carla Vogt, ED - Rainer Wennrich, ED - Gerhard Werner, T1 - Elementspurenanalytik an höchstreinen Säuren mit GF-AAS und mit HR-ICP-MS T2 - CANAS `97 - Colloquium Analytische Atomspektroskopie CY - Freiberg, Deutschland DA - 1997-03-09 KW - GF-AAS KW - Anreicherung im Graphitrohr KW - HR-ICP-MS KW - Reinstsäuren KW - Subboiling-Destillation PY - 1998 SN - 0945-2524 SP - 421 EP - 430 CY - Leipzig AN - OPUS4-15830 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heinrich, Hans-Joachim A1 - Matschat, Ralf T1 - Investigations on Freon-assisted atomization of refractory analytes (Cr, Mo, Ti, V) in multielement electrothermal atomic absorption spectrometry N2 - Premixed 1% Freon in argon inner gas of various composition (CCl2F2, CHClF2, CHF3) was applied to graphite furnace atomizer to minimize unfavorable effects of carbide formation, such as signal tailing and memory effects in the simultaneous determination of Cr, Mo, Ti and V refractory analytes by electrothermal atomic absorption spectrometry using a multielement atomic absorption spectrometer. The effect of these gaseous additives was investigated when applied separately in atomization, pyrolysis and clean-out steps. The halogenation effects were analytically useful only under the precondition of using Ar–H2 outer gas to the furnace to all heating steps, and also using this gas in the pre-atomization (drying, pyrolysis) steps. Optimum analytical performance was obtained when mixtures of 1% Freon in argon were applied just before and during the atomization step at a flow rate of 50 mL min- 1 and 2% hydrogen was used as purge gas. Using optimum conditions, signal tailings and carry-over contamination were reduced effectively and good precision (relative standard deviation below 1%) could be attained. Applying 1% CHClF2 and an atomization temperature of 2550 °C, the characteristic masses obtained for simple aqueous solutions were 8.8 pg for Cr, 17 pg for Mo, 160 pg for Ti, and 74 pg for V. The limits of detection were 0.05, 0.2, 2.3 and 0.5 µg L- 1 for Cr, Mo, Ti and V, respectively. The developed method was applied to the analysis of digests of advanced ceramics. The accuracy of the procedure was confirmed by analyzing the certified reference material ERM-ED 102 (Boron Carbide Powder) and a silicon nitride powder distributed in the inter-laboratory comparison CCQM-P74. KW - Electrothermal atomic absorption spectrometry KW - Refractory analytes KW - Carry-over contamination KW - Halogenation KW - Freon PY - 2007 DO - https://doi.org/10.1016/j.sab.2007.06.006 SN - 0584-8547 SN - 0038-6987 VL - 62 IS - 8 SP - 807 EP - 816 PB - Elsevier CY - Amsterdam AN - OPUS4-15833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - Untersuchungen zur Multielement-Spurenanalytik von Siliciumnitridpulver durch Mikrowellen-Druckaufschluss und atomspektrometrische Detektion T2 - CANAS '99, Colloquium Analytische Atomspektroskopie CY - Konstanz, Germany DA - 1999-03-14 PY - 1999 AN - OPUS4-15936 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - Einsatz unterschiedlicher atomspektrometrischer Methoden und Techniken zur Elementspurenanalytik ausgewählter Reinststoff-Kalibriersubstanzen T2 - Analytica '96 CY - Munich, Germany DA - 1996-04-23 PY - 1996 AN - OPUS4-16010 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - Rückführbare Messungen zur Multielement-Spurenbestimmung in reinen Metallen mit dem neuen Glimmentladungs-Massenspektrometer Element-GD T2 - GDMB-Hauptsitzung CY - Geisenheim, Germany DA - 2007-11-06 PY - 2007 AN - OPUS4-16213 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - BAM system of primary pure standards for elemental analysis - potential contributions of GD-MS calibrated in a new traceable way T2 - Herbstsitzung der IAWG des CCQM am NIST CY - Charleston, SC, USA DA - 2007-10-01 PY - 2007 AN - OPUS4-16215 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schiel, D. A1 - Rienitz, O. A1 - Jährling, R. A1 - Güttler, B. A1 - Matschat, Ralf A1 - Scharf, Holger A1 - Birkhahn, Jürgen A1 - Labarraque, G. A1 - Fisicaro, P. A1 - Borchers, U. A1 - Schwesig, D. T1 - Metrological concept for comparable measurement results under the European water framework directive: demonstration of its applicability in elemental analysis N2 - Within the scope of a project of the 'European Association of National Metrology Institutes' (EURAMET), a European metrological dissemination System (network) providing traceable reference values assigned to matrix materials for validation purposes is described and put to the test. It enables testing laboratories (TL) to obtain comparable results for measurements under the 'EU Water Framework Directive 2000/60/EC' (WFD) and thus, to comply with a core requirement of this very directive. The dissemination system is characterized by the fact that it is available to all laboratories throughout Europe which intend to perform measurements in the context of the WFD and that it can ensure sustainable metrological traceability to the International System of Units (SI) as a reference point for the measurement results. This Dissemination system is set up in a hierarchical manner and links up the level of the national metrology institutes (NMI) with that of the TLs via an intermediate level of calibration laboratories (CL) by comparison measurements. The CLs are expert laboratories with respect to the measurement of the analytes considered here (within the project, the CLs are called potential calibration laboratories (PCL)) and are additionally involved in the organization of comparison measurements within the scope of regional quality assurance (QA) systems. Three comparison measurements have been performed to support the approach. A total of about 130 laboratories participated in this exercise with the focus on the measurement of the priority substances Pb, Cd, Hg, and Ni defined in the WFD. The elemental concentrations in the water samples roughly corresponded to one of the established environmental quality standards (EQS), the annual average concentration (AA-EQS), which is defined in the daughter Directive 2008/105/EC of the WFD. It turned out that a significant number of TLs still need to improve their measurement methods in order to be able to fulfill the Minimum requirements of the WFD, in particular, with regard to the elements Cd and Hg probably due to their low EQS values. Furthermore, it became obvious that the hierarchical Dissemination system suggested here actually corresponds to the measuring capabilities of the three participating Groups (NMIs, PCLs, and TLs). KW - Metrology KW - Metrological traceability KW - Comparability KW - Elemental analysis KW - Water framework directive PY - 2011 DO - https://doi.org/10.1007/s00769-011-0792-z SN - 0949-1775 SN - 1432-0517 VL - 16 IS - 10 SP - 489 EP - 498 PB - Springer CY - Berlin AN - OPUS4-24485 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Dudzus, Thomas A1 - Meier, Klaus A1 - Recknagel, Sebastian A1 - Hedrich, Martina A1 - Matschat, Ralf T1 - Measurement of oxygen and nitrogen in high purity metals used as national standards for elemental analysis in Germany by classical carrier gas hot extraction (HE) and HE after activation with photons N2 - The special importance of the analysis of non-metals in high purity metals, which will serve as national standards for elemental analysis in Germany, is illustrated for oxygen and nitrogen. The typical range of the mass fraction of oxygen and nitrogen in these materials is below 10.MU.g/g, often close to 1.MU.g/g. The two methods applied at BAM for these measurements are classical carrier gas hot extraction (HE) and carrier gas hot extraction after activation with photons (PAA-HE). The approach, the methods and their advantages and limitations are discussed. Comparative results from the measurement of oxygen and nitrogen in Cu, Fe, Ga, Pb, Sn and W are presented. (author abst.) T2 - 8th International Conference on Ultra-High Purity Base Metals (UHPM-2001) CY - Berlin, Germany DA - 2001-06-25 KW - Oxygen determination KW - Nitrogen determination KW - High purity metals KW - Carrier gas hot extraction KW - Photon activation analysis PY - 2002 DO - https://doi.org/10.2320/matertrans.43.98 SN - 1345-9678 SN - 1347-5320 VL - 43 IS - 2 SP - 98 EP - 100 PB - Japan Institute of Metals CY - Sendai AN - OPUS4-1361 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Kuxenko, Sandra A1 - Matschat, Ralf T1 - Auf dem Weg zu rückführbaren Standards für die Elementanalytik - Element-Spurenanalyse in Reinstkupfer KW - Reinstkupfer KW - Elementspurenanalytik KW - Standards KW - Rückführbarkeit PY - 2002 SN - 0016-3538 IS - 6 SP - 718 EP - 720 PB - GIT-Verlag CY - Darmstadt AN - OPUS4-1452 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf T1 - Development of SI-traceable standards of high metrological quality for chemical analysis of the elements T2 - 12th Euroanalysis ; 12th European Conference on Analytical Chemistry CY - Dortmund, Germany DA - 2002-09-08 PY - 2002 SN - 1618-2642 SN - 1618-2650 VL - 375 IS - 8, P1-018 SP - 198 PB - Springer CY - Berlin AN - OPUS4-1630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kipphardt, Heinrich A1 - Matschat, Ralf T1 - Development of SI-traceable standards of high metrological quality for chemical analysis of the elements T2 - Towards an integrated infrastructure for measurements CY - Warszawa, Poland DA - 2002-06-18 PY - 2002 SP - 66 EP - 67 AN - OPUS4-1631 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf A1 - Kipphardt, Heinrich T1 - BAM System of Primary Pure Elements - Aim and Current State T2 - CCQM Annual Meeting of Inorganic Working Group CY - Ottawa, Canada DA - 2002-10-09 PY - 2002 AN - OPUS4-1603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kipphardt, Heinrich A1 - Dudzus, Thomas A1 - Meier, Klaus A1 - Recknagel, Sebastian A1 - Hedrich, Martina A1 - Matschat, Ralf T1 - The measurement of O and N by classical carrier gas hot extraction (HE) - Carrier gas hot extraction after activation with photons T2 - CENAM CY - Mexico City, Mexico DA - 2002-01-28 PY - 2002 AN - OPUS4-1610 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kipphardt, Heinrich A1 - Matschat, Ralf T1 - Preparation of primary calibration substances - method development for trace analysis T2 - CENAM CY - Mexico City, Mexico DA - 2002-01-28 PY - 2002 AN - OPUS4-1611 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matschat, Ralf A1 - Czerwensky, Michael A1 - Pattberg, S. A1 - Heinrich, Hans-Joachim A1 - Tutschku, S. T1 - High Purity Metals as Primary Calibration Materials for Elemental Analysis - Their Importance and Their Certification N2 - The Bundesanstalt fuer Materialforschung und -pruefung, BAM (Federal Institute for Materials Research and Testing) continues to establish a system of primary reference materials to meet the demands of metrological traceability. The materials act as national standards in the field of elemental analysis. For all elements of the periodic table -excepting those that are gases or radioactive- two different kinds of reference materials are being certified. The substances are of very high purity and of defined stoichiometry. Pure elements and metals are used as far as possible. They are certified by determining the trace contents of most elements of the periodic table at very low levels using different trace element analysis methods. Recent application of these methods is described and examples of the certification of some pure metals (copper, iron and lead) are given. (author abst.) T2 - 8th International Conference on Ultra-High Purity Base Metals (UHPM-2001) CY - Berlin, Germany DA - 2001-06-25 KW - Trace elemental analysis KW - Atomic spectrometry KW - High purity metals KW - Certification KW - Primary calibration materials KW - Reference materials KW - National standards PY - 2002 UR - https://www.researchgate.net/publication/235927297_High_purity_metals_as_primary_calibration_materials_for_elemental_analysis_-_Their_importance_and_their_certification SN - 1345-9678 SN - 1347-5320 VL - 43 IS - 2 SP - 90 EP - 97 PB - Japan Institute of Metals CY - Sendai AN - OPUS4-1600 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf A1 - Kipphardt, Heinrich A1 - Recknagel, Sebastian A1 - Noack, Siegfried ED - Abiko, K. ED - Takaki, S. T1 - Activities of Division "Inorganic Chemical Analysis; Reference Materials" of BAM in the Field of Analysis of Metals T2 - 9th international conference on ultrahigh-purity base metals CY - Sendai, Japan DA - 2002-10-14 PY - 2002 SP - 297 EP - 302 CY - Sendai AN - OPUS4-1602 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Matschat, Ralf A1 - Dudzus, Thomas A1 - Meier, Klaus A1 - Recknagel, Sebastian A1 - Kipphardt, Heinrich A1 - Hedrich, Martina ED - Hirschfeld, D. T1 - Messung von Sauerstoff und Stickstoff mit klassischer Trägergasheißextraktion und Trägergasheißextraktion nach Aktivierung mit Photonen für die nationalen primären Kalibriernormale T2 - 8. Symposium Nichtmetalle in Metallen - NIM ; 8. Tagung des Gemeinschaftsausschusses "Nichtmetalle in Metallen" der GDMB CY - Münster, Deutschland DA - 2000-03-16 PY - 2000 SN - 3-9806913-1-4 SP - 19 EP - 27 PB - GDMB, Ges. für Bergbau, Metallurgie, Rohstoff- und Umwelttechnik CY - Clausthal-Zellerfeld AN - OPUS4-915 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gopala, Anil A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Process methodology for the small scale production of m6N5 purity zinc using a resistance heated vacuum distillation system N2 - Ultra high purity Zn (m6N5) was obtained through triple vacuum distillation using an m4N5 Zn as input material. High-volatile impurities were removed from the zinc matrix by vacuum evaporation, while traces having lower volatility than the matrix remained in the residual material after finishing of the entire purification process. The time required for the removal of the main high-volatile impurity (Cd) was monitored using a connected gas source mass spectrometer. During distillation the Zn vapor of the distillate was condensed on the cap of a glassy carbon crucible which was water cooled by a movable copper block. The temperatures were optimized for the removal of the volatiles and for the distillation process using vapor pressure data. High resolution glow discharge mass spectrometry was applied for the analysis and purity evaluation of the distilled and input zinc. The analysis confirmed the reduction of the metallic impurities from 43 mg kg-1 to 0.5 mg kg-1 (m6N5) after three consecutive vacuum distillations. An increase in the grain size and a decrease in the micro-hardness were observed for the purified Zn material. KW - Ultra high purity KW - Vacuum distillation KW - High resolution glow discharge mass KW - Spectrometry KW - Micro-hardness KW - Zinc KW - Purification PY - 2010 DO - https://doi.org/10.1016/j.matchemphys.2010.02.080 SN - 0254-0584 VL - 122 IS - 1 SP - 151 EP - 155 PB - Elsevier CY - Amsterdam AN - OPUS4-21127 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matschat, Ralf A1 - Haßler, J. A1 - Traub, Heike A1 - Dette, Angelika T1 - Multielement trace determination in SiC powders: assessment of interlaboratory comparisons aimed at the validation and standardization of analytical procedures with direct solid sampling based on ETV ICP OES and DC arc OES N2 - The members of the committee NMP 264 Chemical analysis of non-oxidic raw and basic materials of the German Standards Institute (DIN) have organized two interlaboratory comparisons for multielement determination of trace elements in silicon carbide (SiC) powders via direct solid sampling methods. One of the interlaboratory comparisons was based on the application of inductively coupled plasma optical emission spectrometry with electrothermal vaporization (ETV ICP OES), and the other on the application of optical emission spectrometry with direct current arc (DC arc OES). The interlaboratory comparisons were organized and performed in the framework of the development of two standards related to the determination of mass fractions of metallic impurities in powders and grain sizes of ceramic raw and basic materials by both methods. SiC powders were used as typical examples of this category of material. The aim of the interlaboratory comparisons was to determine the repeatability and reproducibility of both analytical methods to be standardized. This was an important contribution to the practical applicability of both draft standards. Eight laboratories participated in the interlaboratory comparison with ETV ICP OES and nine in the interlaboratory comparison with DC arc OES. Ten analytes were investigated by ETV ICP OES and eleven by DC arc OES. Six different SiC powders were used for the calibration. The mass fractions of their relevant trace elements were determined after wet chemical digestion. All participants followed the analytical requirements described in the draft standards. In the calculation process, three of the calibration materials were used successively as analytical samples. This was managed in the following manner: the material that had just been used as the analytical sample was excluded from the calibration, so the five other materials were used to establish the calibration plot. The results from the interlaboratory comparisons were summarized and used to determine the repeatability and the reproducibility (expressed as standard deviations) of both methods. The calculation was carried out according to the related standard. The results are specified and discussed in this paper, as are the optimized analytical conditions determined and used by the authors of this paper. For both methods, the repeatability relative standard deviations were <25%, usually ~10%, and the reproducibility relative standard deviations were <35%, usually ~15%. These results were regarded as satifactory for both methods intended for rapid analysis of materials for which decomposition is difficult and time-consuming. Also described are some results from an interlaboratory comparison used to certify one of the materials that had been previously used for validation in both interlaboratory comparisons. Thirty laboratories (from eight countries) participated in this interlaboratory comparison for certification. As examples, accepted results are shown from laboratories that used ETV ICP OES or DC arc OES and had performed calibrations by using solutions or oxides, respectively. The certified mass fractions of the certified reference materials were also compared with the mass fractions determined in the interlaboratory comparisons performed within the framework of method standardization. Good agreement was found for most of the analytes. KW - Inductively coupled plasma optical emission spectrometry KW - Electrothermal vaporization KW - ETV ICP OES KW - Direct current optical emission spectrometry KW - DC arc OES KW - Direct solid sampling technique KW - Silicon carbide powder KW - Method validation KW - Method standardization KW - Direkte Feststoffanalytik KW - Normung KW - Methodenvalidierung KW - Ringversuche KW - Siliciumcarbid PY - 2005 DO - https://doi.org/10.1007/s00216-005-3415-x SN - 1618-2642 SN - 1618-2650 VL - 383 IS - 7-8 SP - 1060 EP - 1074 PB - Springer CY - Berlin AN - OPUS4-10890 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - Investigation of a transparent glass ceramics concerning the identification as a strange material in glass cullet T2 - Meeting international Commission in Glas (ICG) - Technical Committee 2 (TC-2) CY - Berlin, Germany DA - 2006-04-27 PY - 2006 AN - OPUS4-12383 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lange, Britta A1 - Recknagel, Sebastian A1 - Czerwensky, Michael A1 - Matschat, Ralf A1 - Michaelis, Matthias A1 - Peplinski, Burkhard A1 - Panne, Ulrich T1 - Analysis of pure copper - a comparison of analytical mehods KW - Pure copper KW - Elemental analytical mehtods KW - Reference material KW - Sample dissolution PY - 2008 DO - https://doi.org/10.1007/s00604-007-0849-1 SN - 0026-3672 SN - 1436-5073 VL - 160 SP - 97 EP - 107 PB - Springer CY - Wien AN - OPUS4-17565 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Metrology in chemistry - a rocky road N2 - The application of metrology in chemical analysis is today hampered by psychological and practical barriers. The argumentation is based on the differences in physical and chemical metrology, which arises mainly from the objects of the measurements. The term “measurement” is discussed in the realm of analytical chemistry with a special focus on the inherent relation between chemical identification and determination as well as the consequent use of the concept of traceability and uncertainty. KW - Metrology in chemistry KW - Chemical analysis KW - Traceability KW - Uncertainty PY - 2008 DO - https://doi.org/10.1007/s00604-007-0909-6 SN - 0026-3672 SN - 1436-5073 VL - 162 IS - 1-2 SP - 35 EP - 41 PB - Springer CY - Wien AN - OPUS4-17727 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gusarova, Tamara A1 - Hofmann, T. A1 - Kipphardt, Heinrich A1 - Venzago, C. A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Comparison of different calibration strategies for the analysis of zinc and other pure metals by using the GD-MS instruments VG 9000 and element GD N2 - Synthetic pressed metal powder standards doped with standard solutions were used for the calibration of both commercially available high resolution GD-MS instruments Element GD and VG 9000 for zinc matrix. Different quantification procedures (IBR, Standard RSF, matrix matched RSF from the calibration with CRMs and use of doped synthetic standards) are compared using zinc matrix as an example, whereas the calibration with doped pellets turned out to be the best quantification technique for high-purity materials. The applicability of the Standard RSF concept is scrutinised. In this context, RSF values for several Matrices (Co, Cu, Fe, In and Zn) are reported additionally. PY - 2010 DO - https://doi.org/10.1039/b921649a SN - 0267-9477 SN - 1364-5544 VL - 25 SP - 314 EP - 321 PB - Royal Society of Chemistry CY - London AN - OPUS4-22376 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - Rückführbare Messungen zur Multielement-Spurenbestimmung metallischer und nichtmetallischer Analyten in Reinstmetallen mit dem Glimmentladungs-Massenspektrometer Element-GD T2 - Das 14. Deutsche GDS-Anwendertreffen CY - Berlin, Germany DA - 2008-04-17 PY - 2008 AN - OPUS4-17726 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gopala, Anil A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Use of mass spectrometric detection as a versatile process monitoring tool: reduction patterns in a milled ZnO/Al mixture N2 - Mass spectrometric detection can play a prominent role in the assessment of different reactions occurring at varied temperatures in a milled ZnO/Al mixture. This is the first time that online mass spectrometric information was used as a tool for monitoring and understanding the chemical reduction process mechanism. We have observed four different types of reaction taking place: (1) distillation of Zn metal, (2) reduction of ZnO by activated Al, (3) melting of Al and finally (4) reduction of ZnO by inactivated Al. The experimental conditions and results observed by QMS were supported with literature data and physical measurement data from X-Ray Diffraction (XRD) which gave us an idea about the complex reaction cascade which occurred during the formation of the zinc metal. PY - 2010 DO - https://doi.org/10.1039/c0ay00057d SN - 1759-9660 SN - 1759-9679 VL - 2 SP - 451 EP - 454 PB - RSC Publ. CY - Cambridge AN - OPUS4-21291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Traub, Heike A1 - Wälle, M. A1 - Koch, J. A1 - Panne, Ulrich A1 - Matschat, Ralf A1 - Kipphardt, Heinrich A1 - Günther, D. T1 - Evaluation of different calibration strategies for the analysis of pure copper and zinc samples using femtosecond laser ablation ICP-MS N2 - Solution-doped metal powder pellets as well as aspirated liquids were used as calibration samples to analyze pure copper and zinc certified reference materials (CRMs) by femtosecond laser ablation ICP-MS. It was demonstrated that calibration by copper pellets resulted in relative deviations up to 20%, whereas fs-LA-ICP-MS among copper-based CRMs led to inaccuracies in the same range unless nominal mass fractions were chosen to be <3 mg/kg. Calibration by zinc pellets generally provided better accuracy. Depending on the analyte considered, deviations below 10% were obtained even for mass fractions close to the limit of quantification. Our data, therefore, indicate solution-doped metal powder pellets to be suitable as calibration samples for fs-LA-ICP-MS of metals. Furthermore, the utilization of liquid standards for calibration was found to result in stronger deviations of up to 50% for both copper and zinc samples which, in addition, turned out to be dependent on the plasma conditions. KW - Laser ablation KW - ICP-MS KW - Calibration KW - Copper KW - Zinc KW - Metal PY - 2009 DO - https://doi.org/10.1007/s00216-009-3061-9 SN - 1618-2642 SN - 1618-2650 VL - 395 IS - 5 SP - 1471 EP - 1480 PB - Springer CY - Berlin AN - OPUS4-20402 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Traub, Heike A1 - Czerwensky, Michael A1 - Matschat, Ralf A1 - Kipphardt, Heinrich A1 - Panne, Ulrich T1 - Different calibration strategies for the analysis of pure copper metal by nanosecond laser ablation inductively coupled plasma mass spectrometry N2 - In this work, different calibration strategies for the determination of trace elements in pure copper metal by nanosecond laser ablation ICP-MS were investigated. In addition to certified reference materials (CRMs), pellets of doped copper powder were used for calibration. The micro homogeneity of the CRMs as well as the solution-doped pellets was sufficient to use them as calibration samples in combination with a laser spot size of 200 µm. In contrast, pellets doped with analytes in solid form showed a significant heterogeneity. For most of the investigated analytes and copper CRMs the measured mass fractions were within ± 20% of their certified values when other copper CRMs were used as calibration samples. When solution-doped powder pellets were used as calibration samples a systematic trend towards mass fractions below the certified values was observed for nearly all elements determined in the analysed CRMs. Thermal fractionation effects during the ablation of the solution-doped pellets were suspected as the extent of the fractionation depends on the irradiance, whereas fractionation is reduced at higher irradiance. PY - 2010 DO - https://doi.org/10.1039/b915564c SN - 0267-9477 SN - 1364-5544 VL - 25 IS - 5 SP - 690 EP - 696 PB - Royal Society of Chemistry CY - London AN - OPUS4-21195 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - Special new techniques of atomic spectrometric methods for trace analysis of high purity metals T2 - The 10th International Conference on Ultra-High-purity Metallic-Base Materials UHPM 2003 CY - Saint-Étienne, France DA - 2003-06-16 PY - 2003 AN - OPUS4-3717 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - Bewertung von Ringversuchen zur Validierung und Normung von direkten Feststoff-Analysenverfahren zur Multielement-Spurenbestimmung in SiC-Pulvern mit ETV ICP OES und DC Arc OES N2 - Siliciumcarbid (SiC) ist ein wichtiges technisches Material nicht nur in seinen klassischen Anwendungsbereichen, die auf seinen hervorragenden mechanischen Eigenschaften, insbesondere seiner großen Härte, und seinem besonderen thermischen Verhalten beruhen. Vielfache Anwendungen finden sich auch als Hochleistungskeramik, in der Halbleitertechnik, der Opto- und Mikroelektronik. Für seinen Gebrauch in den verschiedenen Anwendungsgebieten ist die Reinheit des Materials von großer Bedeutung. Die auf der Verwendung von Aufschlusslösungen basierende Analytik ist wegen des erforderlichen zeitaufwendigen Aufschlussverfahrens wenig effektiv. Für größere Analysenserien und für die schnellere Bereitstellung der Ergebnisse sind deshalb direkte Analysenverfahren mit Festprobentechnik von verschiedenen Autoren erprobt und eingesetzt worden. Um zu zuverlässigen und vergleichbaren analytischen Aussagen zu gelangen, sind für einen breiten Einsatz bei den Herstellern validierte und genormte Analysenverfahren erforderlich. Die vorgestellten Ergebnisse sind Bestandteil des Validierungs- und Normungsprozesses. Hierbei wurde für jede der beiden Feststoff-Analysenmethoden mit Multielementcharakter, die optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma und elektrothermischer Verdampfung (ETV ICP OES) und die optische Emissionsspektrometrie mit Gleichstrombogenanregung (DC Arc OES), ein Ringversuch zur Multielement-Spurenbestimmung an sechs vorcharakterisierten Siliciumcarbidpulvern durchgeführt. An diesen Laborvergleichen beteiligten sich mit der ETV ICP OES acht und mit der DC Arc OES neun Laboratorien aus Industrieunternehmen, Forschungseinrichtungen und Universitäten. An jeder der sechs untersuchten Proben wurden sechs parallele Messungen ausgeführt, mit der ETV ICP OES für die Analyten Al, Ca, Cr, Cu, Fe, Mg, Ni, Ti, V und Zr und mit der DC Arc OES für die Analyten Al, B, Ca, Fe, Mg, Ni, Ti und Zr. Für drei der sechs Proben wurden die Gehalte aus den auf der Basis dieser Messungen bestimmten Kalibrierkurven ermittelt, wobei die jeweilige Probe nicht in die Kalibrierung einbezogen wurde. Aus den ermittelten Gehalten wurden nach DIN ISO 5725-2 die Wiederhol- und die Vergleichspräzision beider Analysenverfahren berechnet. Diese stellen wichtige Beiträge zur Verfahrensvalidierung und zur geplanten Normung im Rahmen des DIN NMP 264 "Chemische Analyse von nichtoxidischen keramischen Roh- und Werkstoffen" dar. Ein Eindruck über die Richtigkeit beider Analysenverfahren läßt sich durch Vergleich der Ergebnisse mit den durch rückführbare Messungen zuvor erhaltenen Werten gewinnen. Dabei ist zu beachten, dass diese auch für die Kalibrierung verwendeten Gehaltsangaben der sechs verschiedenen Kalibrierproben nicht in allen Fällen auf einer geraden oder monoton steigenden Kalibrierkurve liegen. Im Nachgang wurde außerdem von der BAM in Kooperation mit der GDMB und unter breiter internationaler Beteiligung eines der sechs SiC-Pulver als Referenzmaterial zertifiziert. Hierdurch wird die Zuverlässigkeit der Aussagen zur Richtigkeit noch weiter erhöht. Die Vergleichs- und die Wiederholpräzision werden als überwiegend gut eingeschätzt, die Richtigkeit als gut bis befriedigend; nur in wenigen Fällen treten größere systematische Abweichungen von den Referenzwerten auf. Damit werden beide Analysentechniken als geeignet zur schnellen Direktanalytik der nur schwer und zeitaufwendig aufzuschließenden Siliciumcarbidpulver bewertet. Im Beitrag wird außer auf die Ringversuche und ihre Auswertung auch auf methodische Besonderheiten beider direkten Feststoff-Analysenverfahren eingegangen. T2 - CANAS '05, Colloquium Analytische Atomspektroskopie CY - Freiberg, Germany DA - 2005-03-06 PY - 2005 AN - OPUS4-6253 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matschat, Ralf A1 - Czerwensky, Michael A1 - Traub, Heike A1 - Heinrich, Hans-Joachim A1 - Kipphardt, Heinrich T1 - Special new techniques of atomic spectrometric methods for trace analysis of high purity metals PY - 2003 SN - 0032-6895 SN - 1778-3771 VL - 91 IS - Décembre SP - 37 EP - 50, N° Hors Série CY - Paris AN - OPUS4-6188 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - Application of different analytical methods for the multi-element ultra-trace dertermination in ultrahigh purity metals T2 - 14th Conference on Ultrahigh Purity Metals CY - Paris, France DA - 2007-07-02 PY - 2007 AN - OPUS4-14947 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Traub, Heike A1 - Czerwensky, Michael A1 - Matschat, Ralf A1 - Kipphardt, Heinrich A1 - Panne, Ulrich T1 - Homogenitätsprüfung und Analyse von reinem Kupfer mit Laserablation-ICP-Massenspektrometrie KW - Laserablation KW - Kupfer KW - Homogenität KW - ZRM PY - 2007 SN - 0026-0746 VL - 61 IS - 11 SP - 744 EP - 745 PB - Giesel Verlag GmbH CY - Isernhagen AN - OPUS4-16153 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - Multielement-Spurenbestimmung in Reinstmetallen und in Reinstmedien der Miktroelektronik mit massenspektrometrischen Methoden T2 - 21. ICP-MS Anwendertreffen und 8. Symposium über Massenspektrometrische Verfahren der Elementspurenanalyse CY - Dresden, Germany DA - 2008-09-17 PY - 2008 AN - OPUS4-17721 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wienold, Julia A1 - Traub, Heike A1 - Lange, Britta A1 - Giray, Thorsten A1 - Recknagel, Sebastian A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Elemental analysis of copper and magnesium alloy samples using IR-laser ablation in comparison with spark and glow discharge methods N2 - Three methods for direct solid sampling of bulk material namely IR laser ablation, glow discharge and spark OES, were compared with respect to analytical figures of merit obtained for elemental analysis with atomic spectrometry. Matrices investigated were copper, pressed doped copper powder, and magnesium alloys. For the vast majority of analytes, statistical equivalence regarding precision (usually ≤ 5%) and the performance of the calibrations between the compared methods was demonstrated. KW - LA-ICP-MS KW - GD-MS KW - Spark-OES KW - LA-ICP-OES KW - Copper KW - Magnesium PY - 2009 DO - https://doi.org/10.1039/b903251g SN - 0267-9477 SN - 1364-5544 VL - 24 SP - 1570 EP - 1574 PB - Royal Society of Chemistry CY - London AN - OPUS4-20257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hommel, C. A1 - Hassler, J. A1 - Matschat, Ralf A1 - Vogt, T. A1 - Detcheva, A. K. A1 - Recknagel, Sebastian T1 - A fast and robust direct solid sampling method for the determination of 27 trace, main and minor elements in soda-lime glass based on ETV-ICP OES and using a gaseous halogenating modifier N2 - A method, based on electrothermal vaporization (ETV) coupled to inductively coupled plasma optical emission spectrometry (ICP OES), has been optimized for direct solid sampling analysis of soda-lime glass - the most common type of industrially manufactured glass. This method allows fast and reliable quantification of the main elements - Al, Ca, K, Mg, Na, and Si - and trace elements - As, Ba, Cd, Ce, Co, Cr, Cu, Fe, Mn, Mo, Ni, (P), Pb, Sb, (Se), Sn, Sr, Ti, V, Zn, and Zr. In the presented ETV-ICP OES method, calibration is performed predominantly with matrix-free synthetic samples. This metrological advantage is normally not achieved with direct solid sampling methods and is one of the goals of the present study. In a certification interlaboratory comparison for the soda-lime glass CRM BAM-S005c, 2 out of 16 laboratories employed the ETV-ICP OES method. An improved analytical performance was obtained compared with the results of laboratories that used conventional liquid ICP OES. For both methods, the average relative deviations between the laboratory results and certified values as well as the average values of relative standard deviation were with a few exceptions <10%, in most cases even <5%, which indicated high trueness and precision. KW - ICP-OES KW - ETV KW - Soda-lime glass KW - Reference material PY - 2021 DO - https://doi.org/10.1039/d1ja00081k SN - 0267-9477 SN - 1364-5544 VL - 36 IS - 8 SP - 1683 EP - 1693 PB - Royal Society of Chemistry CY - London AN - OPUS4-53181 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matschat, Ralf A1 - Czerwensky, Michael A1 - Kuxenko, Sandra A1 - Heinrich, Hans-Joachim T1 - Certification of high purity metals as primary reference materials - a challenge for multielement trace analysis N2 - The Bundesanstalt für Materialforschung und -prüfung (Federal Institute for Materials Research and Testing) (BAM) is establishing a system of primary reference materials to meet the demands for metrological traceability and to act as national standards in the field of elemental analysis. For all elements of the periodic table - except those that are gases or radioactive - two different kinds of reference materials are being certified. One is for analyte calibration (Type A) and one for problems concerning matrix matching (Type B). These substances are of very high purity and of defined stoichiometry. As far as possible, pure elements and metals rather than pure compounds are used. The certification of both types of material requires most elements of the periodic table to be certified at very low levels using trace element analysis methods. The application of these methods is described and examples of the certification of copper and iron are given. KW - Elementspurenanalytik KW - Primäre Referenzmaterialien PY - 2002 DO - https://doi.org/10.1002/1521-396X(200201)189:1%3C107::AID-PSSA107%3E3.0.CO;2-1 SN - 1862-6300 SN - 0031-8965 N1 - Geburtsname von Kuxenko, Sandra: Pattberg, S. - Birth name of Kuxenko, Sandra: Pattberg, S. VL - 189 IS - 1 SP - 107 EP - 122 PB - Wiley-VCH CY - Berlin AN - OPUS4-837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matschat, Ralf A1 - Richter, Silke A1 - Vogl, Jochen A1 - Kipphardt, Heinrich T1 - On the way to SI traceable primary transfer standards for amount of substance measurements in inorganic chemical analysis N2 - During its 25 years of existence, the Inorganic Analysis Working Group of the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM IAWG) has achieved much in establishing comparability of measurement results. Impressive work has been done on comparison exercises related to real-world problems in fields such as ecology, food, or health. In more recent attempts, measurements and comparisons were focused on calibration solutions which are the basis of most inorganic chemical measurements. This contribution deals with the question of how to achieve full and transparent SI traceability for the values carried by such solutions. Within this framework, the use of classical primary methods (CPMs) is compared to the use of a primary difference method (PDM). PDM is a method with a dual character, namely a metrological method with a primary character, based on the bundling of many measurement methods for individual impurities, which lead to materials with certified content of the main component. As in classical methods, where small corrections for interferences are accepted, in PDM, many small corrections are bundled. In contrast to classical methods, the PDM is universally applicable to all elements in principle. Both approaches can be used to certify the purity (expressed as mass fraction of the main element) of a high-purity material. This is where the metrological need of National Metrology Institutes (NMIs) for analytical methods meet the challenges of analytical methods. In terms of methods, glow discharge mass spectrometry (GMDS) with sufficient uncertainties for sufficiently small impurity contents is particularly noteworthy for the certification of primary transfer standards (PTS), and isotope dilution mass spectrometry (IDMS), which particularly benefits from PTS (back-spikes) with small uncertainties, is particularly noteworthy for the application. The corresponding relative uncertainty which can be achieved using the PDM is very low (< 10−4). Acting as PTS, they represent the link between the material aspect of the primary calibration solutions and the immaterial world of the International System of Units (SI). The underlying concepts are discussed, the current status of implementation is summarised, and a roadmap of the necessary future activities in inorganic analytical chemistry is sketched. It has to be noted that smaller measurement uncertainties of the purity of high-purity materials not only have a positive effect on chemical measurements, but also trigger new developments and findings in other disciplines such as thermometry or materials science. KW - Inorganic chemical analysis KW - Primary transfer standards (PTSs) KW - Traceability KW - Classical primary measurement method (CPM) KW - Primary difference measurement method (PDM) KW - Metrology in chemistry PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572743 DO - https://doi.org/10.1007/s00216-023-04660-4 SN - 1618-2642 SN - 1618-2650 VL - 415 SP - 3057 EP - 3071 PB - Springer CY - Berlin AN - OPUS4-57274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - The System of Primary Pure Metals Establisted at BAM - Recent Developments T2 - The 9th International Conference on Ultra-High-Purity Base Metals CY - Sendai, Japan DA - 2002-10-13 PY - 2002 AN - OPUS4-2937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hassler, J. A1 - Barth, P. A1 - Richter, Silke A1 - Matschat, Ralf T1 - Determination of trace elements in high-purity copper by ETV-ICP OES using halocarbons as chemical modifiers N2 - Inspired by the globule arc technique a new electrothermal vaporization inductively coupled plasma optical emission spectrometry (ETV-ICP OES) method was developed for the analysis of high-purity copper materials. The performance of the method was investigated for the analytes Ag, Al, As, Bi, Cd, Co, Cr, Fe, Mg, Mn, Ni, P, Pb, S, Sb, Se, Si, Sn, Te, Ti, Zn and Zr. ETV parameters were optimized regarding the release of the analytes, the transport efficiency and the quality of analytical results in terms of precision, trueness and power of detection. The influence of CCl2F2, CHClF2, C2H2F4 and CHF3 as gaseous halogenation modifiers was investigated. A sufficient in situ analyte matrix separation was achieved by using CHF3 as halogenating reagent avoiding a high matrix input from the molten copper sample into the ETV system and the plasma. A complete release from the samples was obtained for all investigated analytes except Se and Te. Acceptable results for the determination of the trace elements Ag, Al, As, Bi, Cd, Co, Cr, Fe, Mg, Mn, Ni, P, Pb, S, Sb, Si, Sn, Ti, Zn and Zr in high-purity copper were achieved. The method includes a preceding sample preparation step of oxidizing the surface of copper samples which results in a significantly enhanced sensitivity. In addition to the calibration with copper samples, the feasibility of the calibration with liquid multi-element solutions was investigated. Except for Ag, Mg and Ni all analytes could be analyzed using aqueous calibration solutions. The trueness of the method was tested by the determination of analyte contents of certified reference materials. Limits of quantification ranging from 0.6 ng g-1 to 29 ng g-1 were achieved. The developed direct solid sampling method is time and cost effective and well suited for the characterization of high-purity copper materials. The method can be automated to a large extent and is applicable for processes accompanying analyses. In contrast to all other investigated trace elements, Se and Te were not released from the matrix at measurable levels under the used conditions. The determination of these elements is still under investigation and will be reported in a succeeding publication. KW - ETV KW - Copper KW - Impurities PY - 2011 DO - https://doi.org/10.1039/c1ja10149h SN - 0267-9477 SN - 1364-5544 VL - 26 IS - 12 SP - 2404 EP - 2418 PB - Royal Society of Chemistry CY - London AN - OPUS4-29615 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhou, T. A1 - Richter, Silke A1 - Matschat, Ralf A1 - Kipphardt, Heinrich T1 - Determination of the total purity of a high-purity silver material to be used as a primary standard for element determination N2 - A candidate material for the use as primary standard for silver determination was characterized with respect to total purity. Except the radioactive elements and He, all possible impurities were considered. Based on glow discharge mass spectrometry, inductively coupled plasma-mass spectrometry and carrier gas hot extraction measurements, the demonstrated total purity and its standard uncertainty is w(Ag) = (99.999 52 ± 0.000 11) %. The purity value and its uncertainty is dominated by the contributions from the measurements of the nonmetallic impurities, namely S, N, C and O. KW - Silver KW - Purity KW - Total purity KW - Primary standard KW - Element determination PY - 2013 DO - https://doi.org/10.1007/s00769-013-0988-5 SN - 0949-1775 SN - 1432-0517 VL - 18 IS - 4 SP - 341 EP - 349 PB - Springer CY - Berlin AN - OPUS4-28971 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gusarova, Tamara A1 - Methven, B. A1 - Kipphardt, Heinrich A1 - Sturgeon, R. A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Calibration of double focusing glow discharge mass spectrometry instruments with pin-shaped synthetic standards N2 - Calibration of two commercially available glow discharge double focusing mass spectrometers, the VG 9000 and Element GD, is described using synthetic pin standards pressed from solution doped copper and zinc matrices. A special pressing die was developed for this purpose and optimal results were obtained with the highest possible pressures, i.e., 95 kN·cm- 2. This calibration approach permits the determination of trace element mass fractions down to µg·kg- 1 with small uncertainties and additionally provides traceability of the GD-MS results in the most direct manner to the SI (International System of Units). Results were validated by concurrent measurements of a number of compact copper and zinc certified reference materials. The impact of the sample pin cross-section (circular or square) was investigated with the use of a new pin-sample holder system for the Element GD. The pin-sample holder was designed by the manufacturer for pin-samples having circular cross-section; however, samples with square pin cross-section were also shown to provide acceptable results. Relative Sensitivity Factors for some 50 analytes in copper (VG 9000, Element GD) and zinc matrices (VG 9000) are presented. The field of applicability of GD-MS may be considerably extended via analysis of pin geometry samples based on their ease of preparation, especially with respect to the accuracy and traceability of the results and the enhanced number of analytes which can be reliably calibrated using such samples. KW - Glow discharge KW - Pin sample KW - Calibration PY - 2011 DO - https://doi.org/10.1016/j.sab.2011.12.001 SN - 0584-8547 SN - 0038-6987 VL - 66 IS - 11-12 SP - 847 EP - 854 PB - Elsevier CY - Amsterdam AN - OPUS4-25346 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gopala, Anil A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Mass spectrometry insight of the process mechanism during the vacuum distillation of zinc N2 - Detection and monitoring of volatile elements released during the preparation of ultra high purity zinc by vacuum distillation (VD) is reported using online quadrupole gas source mass spectrometry (QMS). The theoretically calculated vapour pressures (pv) for the volatile impurity elements using Dushman constants and the practically observed mass spectra were found to be consistent (S. Dushman and J. M. Lafferty, Scienific Foundations of Vacuum Technique, 2nd ed., Wiley, New York, 1962). This is the first time that the potential ability of an online mass spectrometer was used for monitoring and understanding the process mechanism during the purification of metals (Zn) using VD. We here also illustrate our findings with the results from high resolution glow discharge mass spectrometer (HR-GDMS) analysis before and after the purification of Zn. PY - 2009 DO - https://doi.org/10.1039/b904133h SN - 0267-9477 SN - 1364-5544 VL - 24 SP - 887 EP - 890 PB - Royal Society of Chemistry CY - London AN - OPUS4-19595 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Development of SI traceable standards for element determination N2 - In Germany a system of primary amount of substance standards for elemental analysis is being developed, which forms the material´s basis for the National Standards for element determination. The metrological concept and technical approach is briefly described. The objective of traceability in chemistry, in this case for elemental determination, is illustrated on the example of copper. KW - Copper KW - Element determination KW - Metrology KW - Primary standards KW - Traceability PY - 2009 DO - https://doi.org/10.2533/chimia.2009.637 SN - 0009-4293 VL - 63 IS - 10 SP - 637 EP - 639 PB - Schweizerische Chemische Gesellschaft CY - Basel AN - OPUS4-20727 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rudtsch, S. A1 - Gusarova, Tamara A1 - Aulich, A. A1 - Fahr, M. A1 - Fischer, J. A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Procedure for the impurity-related correction at the indium fixed-point N2 - Determining the influence of impurities on the fixed-point emperatures of the ITS-90 requires the completion of several tasks. In this paper, the Progress made at Physikalisch-Technische Bundesanstalt (PTB) and BAMFederal Institute for Materials Research and Testing is presented and remaining questions are discussed. The projected characterization procedure at PTB, which is based on the established SIE method (sum of the individual estimates), using a new indium fixed-point cell is described as an example. This procedure includes an SI-traceable chemical Analysis of the material in the fixed-point cell with sufficiently low uncertainties, the individual experimental determination of the influence of the quantified impurities on the fixed-point temperature, and the establishment of direct links to the phase-transition temperatures of the national standard and of an assumed material of ideal purity. A characteristic difference to the common practice is the chemical analysis of the fixed-point metal being done after determining the cell’s freezing temperature. This allows for the detection and consideration of contamination and purification effects due to the filling process, or due to the contact with the carbon crucible and other parts of the fixed-point cell. A chemical analysis of an indium fixed-point was carried out by BAM with relative measurement uncertainties below 30 % which have not been previously achieved. The results provide evidence for the precipitation of some impurities, which is apparently inconsistent with the corresponding binary phase diagrams, but was explained in a recent publication. Implications for the use of the SIE method shall be described briefly at the end. KW - Chemical analysis KW - Fixed-points KW - Impurities KW - ITS-90 PY - 2011 DO - https://doi.org/10.1007/s10765-011-0915-0 SN - 0195-928X SN - 1572-9567 VL - 32 IS - 1-2 SP - 293 EP - 302 PB - Springer CY - Dordrecht AN - OPUS4-23373 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matschat, Ralf A1 - Hassler, J. A1 - Richter, Silke A1 - Kleve, M. A1 - Dette, A. T1 - Multielement trace analysis of pure graphite powders using optical emission spectrometry coupled to a magnetically stabilized DC arc supplied with halogenating gases as chemical modifiers – a rapid and robust methodology N2 - A magnetically stabilized DC arc device, designed for operation with OES spectrometers was used to determine the elements Ag, Al, B, Ba, Be, Ca, Co, Cr, Cu, Fe, Ga, In, K, Li, Mg, Mn, Mo, Na, Nb, Ni, Si, Sn, Sr, Ti, V, Zr at trace levels of some μg kg−1 up to some 10 mg kg−1 in graphite powders. The coil for the generation of the homogeneous magnetic field was placed outside the closed arc chamber. The time programs of variable current strengths of the magnetic coil (up to 6 A) and of the arc (up to 17 A) which was burning in air were computer controlled. Halogenating gases (mainly CCl2F2, alternatively SF6 and NF3) were used as chemical modifiers to allow an effective release of the carbide forming trace elements. The mass flow controlled modifier gas was led through a special carrier electrode near the arc plasma. The emission radiation was guided by an optical fiber alternatively into two different ICP spectrometers in which the ICP torches were removed. The synergistic interaction of the magnetic field with the halogenating modifier gases resulted in a significant improvement in the analytical performance of the optimized analytical method. All our results for 22 trace elements were in good agreement with the means of an inter-laboratory comparison by BAM for certification of a pure graphite powder material; this holds also for our results for two other graphite materials. The optimized method showed an analytical performance suitable for comprehensive trace analysis of pure graphite. The instrumentation could be integrated into modern DC arc emission spectrometers to improve their analytical capabilities substantially. KW - Graphit KW - DC-Arc KW - High purity KW - Optical emission spectroscopy KW - Magnetically stabilized PY - 2018 DO - https://doi.org/10.1039/C7JA00387K SN - 1364-5544 SN - 0267-9477 VL - 33 IS - 3 SP - 468 EP - 480 PB - Royal Society of Chemistry AN - OPUS4-44398 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hassler, J A1 - Matschat, Ralf A1 - Richter, Silke A1 - Barth, P. A1 - Detcheva, A.K. A1 - Waarlo, H.-J. T1 - Determination of 22 trace elements in high-purity copper including Se and Te by ETV-ICP OES using SF6, NF3, CF4 and H2 as chemical modifiers N2 - In supplementary work to the one published earlier, experiments with SF6, NF3, CF4 and H2 as new modifier gases for the matrix studied were performed. Our investigations were continued to improve the described analytical method and to achieve additional insights into the mechanism of analyte release. Our new survey is split in two parts. At first fluorinating modifiers were used to investigate the behaviour of a variety of trace elements (Ag, Al, As, Au, Bi, Cd, Co, Cr, Fe, Mg, Mn, Ni, P, Pb, Sb, Se, Si, Sn, Te, Ti, Zn and Zr). Most of them (exceptions Au, Se, and Te) could be effectively released from the copper matrix by thermo-halogenation reactions and by partial sub-sample evaporation. Using SF6 and NF3 as modifier gases, low limits of quantification (LOQs) were achieved for the 19 well released trace elements (typical ≤0.1 mg kg-1). Most elements (exceptions Ag, Mg, and Ni) could be calibrated by using aqueous calibration solutions without any sample pretreatment. For the trace determination of Se, Te, and Au, a further analytical method of ETV-ICP OES is described in the second part based on thermo-hydrogenation reactions by using a hydrogen/argon mixture as a modifier gas. The determination of Se and Te with very high analytical performance (LOQ < 0.1 mg kg-1) can either be carried out in a second analytical step succeeding the halogenation procedure, or the sub-sample is directly treated with H2 without previous halogenation procedure whereby the sub-sample can either be partially or totally evaporated. In this case some other analytes (Ag, Au, As, Bi, Cd, Fe, Mg, Ni, Pb, Sb, Sn, and Zn) can additionally be quantified simultaneously with Se and Te. KW - Pure Cu material KW - Electrothermal vaporization KW - Optical-emission spectrometry KW - Plasma-mass-spectrometry KW - Atomic-absorption spectrophotometry KW - Graphite-furnace AAS KW - Pure copper KW - Spectrochemical analysis KW - Precise determination KW - Sample introduction KW - Silicon-carbide PY - 2016 DO - https://doi.org/10.1039/C5JA00240K SN - 0267-9477 SN - 1364-5544 VL - 31 IS - 3 SP - 642 EP - 657 PB - Royal Society of Chemistry CY - London AN - OPUS4-35133 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf T1 - Primäre Kalibriernormale für die metrologische Rückführung in der anorganischen chemischen Analytik T2 - CANAS'03 - Colloquium Analytische Atomspektroskopie CY - Konstanz, Germany DA - 2003-03-23 PY - 2003 AN - OPUS4-3716 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Silke A1 - Meckelburg, Angela A1 - Recknagel, Sebastian A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Determination of trace elements in iron ore, cast iron and steel using the 7500cs KW - Steel KW - Iron ore KW - Cast iron KW - ICP-MS PY - 2009 IS - 38 SP - 4 EP - 5 PB - Agilent Technologies CY - Santa Clara, CA, USA AN - OPUS4-19476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matschat, Ralf A1 - Dette, Angelika A1 - Richter, Silke A1 - Recknagel, Sebastian A1 - Barth, P. T1 - Certification of a boron carbide powder reference material for chemical analysis N2 - The certification of a boron carbide reference material for chemical composition is described. The mass fractions of 16 elements and two boron species are certified in an international interlaboratory comparison with 35 participating laboratories from six different countries. Beside chemical characterization the certification process includes homogeneity and stability testing of the candidate material boron carbide (type F360, 305M422). Details of the analytical methods used for chemical characterization and of the calculation of the uncertainties of the certified mass fractions are given. The new reference material ERM®-ED102 with certified mass fractions of 18 parameters (elements and species) and of the amount fraction of the isotope 10B is a valuable tool for laboratories working in the field of advanced ceramic materials analysis to improve their analytical results. KW - Boron carbide KW - Certified reference material KW - ERM KW - Certification PY - 2011 DO - https://doi.org/10.1111/j.1551-2916.2011.04657.x SN - 0002-7820 SN - 1551-2916 VL - 94 IS - 11 SP - 4009 EP - 4016 PB - Blackwell Publishing CY - Malden AN - OPUS4-24967 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matschat, Ralf A1 - Kipphardt, Heinrich A1 - Czerwensky, Michael A1 - Richter, Silke A1 - Heinrich, Hans-Joachim ED - Abiko, K. ED - Takaki, S. T1 - The System of Primary Pure Metals Established at BAM - Recent Developments T2 - 9th international conference on ultrahigh-purity base metals CY - Sendai, Japan DA - 2002-10-14 PY - 2002 SP - 119 CY - Sendai AN - OPUS4-1601 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gusarova, Tamara A1 - Hodoroaba, Vasile-Dan A1 - Matschat, Ralf A1 - Kipphardt, Heinrich A1 - Panne, Ulrich T1 - Exploitation of the hollow cathode effect for sensitivity enhancement of Grimm-type DC glow discharge optical emission spectroscopy N2 - The hollow cathode (HC) effect was investigated in non-cooled 15 mm deep drilled flat metallic analytical samples that were easy to prepare. The deep cavity used ("complete HC" in contrast to "recessed HC" with 2-3 mm deep cavity) intensified the HC effect notably and therefore distinctly improved the detection power of the common GD-OES with planar cathodes. A signal enhancement of up to a factor of 150, not reported earlier, in comparison with flat conventional samples was achieved. A better separation of the analytical lines from spectral interferences was observed when the HC assembly was applied. Additionally, an effect of strongly enhanced intensities of atomic lines and somewhat decreased intensities of ionic lines was detected in the case of HC in comparison to usual planar cathodes. The investigations were carried out with samples of copper, steel and zinc matrices using both the same and individually optimised glow discharge (GD) electrical parameters. KW - Hollow cathode KW - Grimm type glow discharge KW - Emission spectroscopy KW - GD-OES KW - Sensitivity PY - 2009 DO - https://doi.org/10.1039/b814977a SN - 0267-9477 SN - 1364-5544 VL - 24 SP - 680 EP - 684 PB - Royal Society of Chemistry CY - London AN - OPUS4-19600 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Silke A1 - Roethke, A. A1 - Rienitz, O. A1 - Matschat, Ralf A1 - Schiel, D. A1 - Jaehrling, R. A1 - Goerlitz, V. A1 - Kipphardt, Heinrich T1 - SI-traceable monoelemental solutions on the highest level of accuracy: 25 years from the foundation of CCQM to recent advances in the development of measurement methods N2 - Within the Working Group on Inorganic Analysis (IAWG) of the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM) international key comparisons and pilot studies related to inorganic analysis are carried to ensure consistency in this field at the highest level. Some of these comparisons deal directly with the preparation and characterization of monoelemental solutions or with topics, closely related. The importance of monoelemental solutions lies in the fact that almost every measurement in inorganic analysis relies on the comparison with either a reference material, or references in form of solutions, usually (mono)elemental solutions. All quantitative measurement approaches, e.g. isotope dilution or standard addition, need an accurate reference solution made from a well characterized reference material, prepared under full gravimetric control. These primary (monoelemental) solutions do not only serve as arbitrary references/calibration solutions, but they also link up measurement results to the International System of units (SI), this way establishing the so-called metrological traceability to a measurement unit of the SI. Without such solutions on the highest possible level of accuracy and with the smallest possible associated uncertainties (for e.g. element content and/or impurities), an analysis itself can never be as good as it could be with appropriate reference solutions. This article highlights select key comparisons and pilot studies dealing with monoelemental solution related topics within the IAWG from the foundation of CCQM – 25 years ago – up to latest achievements in the field of inorganic analysis. KW - Metrology KW - SI Traceability KW - CCQM PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-496080 DO - https://doi.org/10.1088/1681-7575/ab5636 SN - 0026-1394 SN - 1681-7575 SP - 1 EP - 23 PB - IOP CY - Bristol AN - OPUS4-49608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Görner, Wolf A1 - Eichelbaum, Maik A1 - Matschat, Ralf A1 - Rademann, K. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich T1 - Non-destructive investigation of composition, chemical properties and structure of materials by synchrotron radiation PY - 2006 SN - 0007-1137 VL - 48 IS - 9 SP - 540 EP - 544 PB - British Institute of Non-Destructive Testing CY - Northampton AN - OPUS4-14186 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peplinski, Burkhard A1 - Fitch, A.N. A1 - Evans, A. A1 - Ibberson, R.M. A1 - Többens, D.M. A1 - Cranswick, L.M.D. A1 - Dörfel, Ilona A1 - Emmerling, Franziska A1 - Matschat, Ralf T1 - Structural characterization of a coarse-grained transparent silicon carbide powder by a combination of powder diffraction techniques N2 - Diffraction of hard synchrotron radiation as well as constant-wavelength and time-of-flight neutron diffraction were used for the structural characterization of a silicon carbide powder having extremely low levels of chemical impurities, high perfection of the crystalline lattice and a grain size of up to 150 µm. The presence of three polytypes was ascertained and the ratios of their mass fractions were determined to be w15R : w6H = 0.002,3(8) and w4H : w6H = 0.000,6(2). KW - Silicon carbide KW - Polytypes KW - Phase quantification KW - Reference material PY - 2009 DO - https://doi.org/10.1524/zksu.2009.0009 SN - 0930-486X VL - 30 EPDIC 2008 SP - 61 EP - 66 PB - Oldenbourg CY - München AN - OPUS4-20561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -